ASTM D4273-18

Standard Test Method for Polyurethane Raw Materials: Determination of Primary Hydroxyl Content of Polyether Polyols

SIGNIFICANCE AND USE
5.1 The primary hydroxyl content provides information about the relative reactivities of polyols.
SCOPE
1.1 Carbon-13 Nuclear Magnetic Resonance Spectroscopy (13C NMR) measures the primary hydroxyl content of ethylene oxide (EO)-propylene oxide (PO) polyether polyols used in preparing flexible polyurethane foams. This method is best suited for polyether polyols with primary hydroxyl contents of 10 to 90 %.  
1.2 The values stated in SI units are to be regarded as standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
Note 1: There is no known ISO equivalent to this standard.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Historical
• Publication Date: 31-Mar-2018
• ICS: 83.080.20 - Thermoplastic materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.22 - Cellular Materials - Plastics and Elastomers

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D4273 − 18
Standard Test Method for
Polyurethane Raw Materials: Determination of Primary
1
Hydroxyl Content of Polyether Polyols
This standard is issued under the fixed designation D4273; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* 3. Terminology
3.1 Definitions—For definitions of terms that appear in this
1.1 Carbon-13 Nuclear Magnetic Resonance Spectroscopy
13
method, refer to Terminology D883 and Practice E2977.
( C NMR) measures the primary hydroxyl content of ethylene
oxide (EO)-propylene oxide (PO) polyether polyols used in
4. Summary of Test Method
preparing flexible polyurethane foams. This method is best
suited for polyether polyols with primary hydroxyl contents of
4.1 Peaks of the primary and secondary hydroxyl carbons of
10 to 90 %.
polyether polyols used in flexible polyurethane foams are
13
well-resolved in high-resolution C NMR spectra. The pri-
1.2 The values stated in SI units are to be regarded as
mary hydroxyl content is determined from the ratio of the
standard.
primary hydroxyl area to the total hydroxyl (primary and
1.3 This standard does not purport to address all of the
secondary) area.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Significance and Use
priate safety, health, and environmental practices and deter-
5.1 The primary hydroxyl content provides information
mine the applicability of regulatory limitations prior to use.
about the relative reactivities of polyols.
NOTE 1—There is no known ISO equivalent to this standard.
6. Interferences
1.4 This international standard was developed in accor-
6.1 Primary hydroxyl PO methylene carbons (where the
dance with internationally recognized principles on standard-
methylene carbon is next to the hydroxyl group and the
ization established in the Decision on Principles for the
methine carbon is next to the ether oxygen) are integrated with
Development of International Standards, Guides and Recom-
the secondary hydroxyl carbons and are therefore not included
mendations issued by the World Trade Organization Technical
in the primary hydroxyl content as measured by this method.
Barriers to Trade (TBT) Committee.
7. Apparatus
2. Referenced Documents
7.1 Fourier-Transform NMR (FT-NMR) Spectrometer, with
2
2.1 ASTM Standards:
carbon-13 capability and a carbon-13 resonance frequency of
D883 Terminology Relating to Plastics
50 MHz (proton resonance frequency of 200 MHz) or higher.
E691 Practice for Conducting an Interlaboratory Study to
The spectrometer is to have a minimum carbon-13 signal-to-
Determine the Precision of a Test Method
noise ratio of 70:1 based on the benzene carbon signal in a
E2977 Practice for Measuring and Reporting Performance of
60 % benzene-d6, 40 % p-dioxane (v/v) sample (ASTM NMR
Fourier-Transform Nuclear Magnetic Resonance (FT-
standard) that has been pulsed once using a 90° pulse angle
NMR) Spectrometers for Liquid Samples
under the conditions specified in Practice E2977.
7.2 NMR sample tubes having outside diameters of 5 mm or
more.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.22 on Cellular Materials -
7.3 NMR spinners.
Plastics and Elastomers.
Current edition approved April 1, 2018. Published April 2018. Originally
8. Reagents and Materials
approved in 1983. Last previous edition approved in 2011 as D4273 - 11. DOI:
10.1520/D4273-18.
8.1 All reagents are to be spectroscopic-grade and free of
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
magnetic materials.
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
8.1.1 Deuterated chloroform or deuterated acetone, con-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. taining tetramethylsilane (TMS) as an internal standard.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D4273 − 18
13
FIG. 1 C NMR Spectrum of an EO-PO Polyol (BB23796)
9. Hazards 12. Procedure
9.1 Magnetic Fields—Follow the manufacturer’s recom- 12.1 Prepare a solution of the polyol sample in deuterated
mendation for the safe operation of the instrument. chloroform or deuterated acetone containing TMS as an
9.1.1 Persons with implanted or attached medical devices internal standard. A 30-60 % solution is recommended. (Se
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4273 − 11 D4273 − 18
Standard Test Method for
Polyurethane Raw Materials: Determination of Primary
1
Hydroxyl Content of Polyether Polyols
This standard is issued under the fixed designation D4273; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope*
13
1.1 Carbon-13 Nuclear Magnetic Resonance Spectroscopy (carbon-13( NMR),C NMR) measures the primary hydroxyl
content of ethylene oxide-propylene oxide polyethers oxide (EO)-propylene oxide (PO) polyether polyols used in preparing
flexible polyurethane foams. It This method is best suited for polyethers polyether polyols with primary hydroxyl contents of 10
to 90 %.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
NOTE 1—There is no known ISO equivalent to this standard.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
3
(Withdrawn 2009)
E386 Practice for Data Presentation Relating to High-Resolution Nuclear Magnetic Resonance (NMR) Spectroscopy
3
(Withdrawn 2015)
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E2977 Practice for Measuring and Reporting Performance of Fourier-Transform Nuclear Magnetic Resonance (FT-NMR)
Spectrometers for Liquid Samples
3. Terminology
3.1 Definitions—The terminology in this test method follows the standard terminology defined in Practice For definitions of
terms that appear in this method, refer to Terminology E386D883 and in Terminology Practice D883E2977.
4. Summary of Test Method
4.1 The resonance peaks Peaks of the primary and secondary hydroxyl carbons of the polyetherspolyether polyols used in
13
flexible urethanepolyurethane foams are well-resolved in high-resolution carbon-13C NMR spectra. The peak areas are measured
by the spectrometer’s integration system, and the relative primary hydroxyl content is determined from the ratio of the primary
hydroxyl area to the total area of the primary and secondary hydroxyl resonance peaks.hydroxyl (primary and secondary) area.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.22 on Cellular Materials - Plastics
and Elastomers.
Current edition approved April 1, 2011April 1, 2018. Published April 2011April 2018. Originally approved in 1983. Last previous edition approved in 20052011 as
D4273 - 05.D4273 - 11. DOI: 10.1520/D4273-11.10.1520/D4273-18.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D4273 − 18
5. Significance and Use
5.1 Measurements of The primary hydroxyl content are useful for providing information regardingprovides information about
the relative reactivities of polyols.
6. Interferences
6.1 Any primary hydroxyl propoxylate carbons present Primary hydroxyl PO methylene carbons (where the methylene carbon
is next to the hydroxyl group and the methine carbon is next to the ether oxygen) are integrated with the secondary hydroxyl
carbons and are therefore not included in the primary hydroxyl content as measured by this method.
7. Equipment
7.1 Pulse Fourier-
...